Summary of the invention
The object of the present invention is to provide a kind of processing method of vacuum induction melting 4J36 low expansion alloy, the method adopts the zirconium white crucible for smelting 4J36 alloy of stabilized with yttrium oxide, effectively can reduce the reaction of alloy liquid and sidewall of crucible, significantly reduce oxide inclusions content; And in fusion process, be filled with argon gas, effectively can reduce collapsing of alloy liquid and spatter, guarantee that alloy liquid is pure, meet service requirements.
Technical scheme of the present invention is: the zirconium white crucible adopting thermodynamically stable stabilized with yttrium oxide, induction melting 4J36 low expansion alloy under malleation argon gas atmosphere, the preparation method of the zirconium white crucible of wherein said stabilized with yttrium oxide is: getting mass percent is that the yttrium oxide powder of 8% and the zirconia powder of 92% carry out mixing rear ball milling, nodularization granulation is carried out after high temperature sintering, and using two acetic acid zirconiums as adhesive cool isostatic pressed forming of green body, eventually pass the zirconium white crucible of the obtained stabilized with yttrium oxide of sintering.
The processing method of vacuum induction melting 4J36 alloy of the present invention, it is characterized in that: before isostatic cool pressing forming of green body, adding CaO particle, (Main Function adding CaO particle reduces crucible sintering temperature as additive, preferred size is 1 ~ 3mm), the weight percent of each composition is: 93 ~ 94% yttrium oxide powder and zirconia powder sintered product, 5%CaO particle, 1 ~ 2% 2 acetic acid zirconium.
The processing method of vacuum induction melting 4J36 alloy of the present invention, concrete steps are as follows:
1) alloy raw material: get pure iron, electrolytic nickel, electrolytic manganese by the massfraction of 4J36 alloy requirement;
2) shove charge in the following order: the zirconium white crucible of stabilized with yttrium oxide put into by electrolytic nickel and pure iron, alloy secondary charging bucket put into by electrolytic manganese, adds after metallization in crucible is clear;
3) malleation is applied: first vacuumized by body of heater, when the low vacuum in stove is in 3Pa, applying argon gas in stove, between plus-pressure to 1000Pa ~ 1500Pa;
4) alloy melting: power transmission, fusing pure iron and electrolytic nickel, in melting process, add electrolytic manganese in the zirconium white crucible of stabilized with yttrium oxide;
5) cast of alloy: all changed by described alloy raw material clearly, between adjustment teeming temperature to 1500 DEG C ~ 1560 DEG C, cast alloy liquid, obtains 4J36 alloy.
Present invention also offers the special copple of described processing method, it is characterized in that, the concrete preparation process of described crucible is as follows:
(1), getting mass percent is that the yttrium oxide powder of 8% and the zirconia powder of 92% mix rear ball milling 3 ~ 4 hours;
(2), adopt high-temperature electric arc melting method to carry out high temperature sintering to gained powder, sintering temperature 1800 DEG C ~ 2800 DEG C, resulting materials carries out nodularization granulation, the oxidation zircon sand of obtained stabilized with yttrium oxide;
(3), in the oxidation zircon sand of stabilized with yttrium oxide add CaO particle, add two acetic acid zirconiums again after both mixing, the weight percent of each composition is: the oxidation zircon sand of 93 ~ 94% stabilized with yttrium oxide, 5%CaO particle, 1 ~ 2% 2 acetic acid zirconium; Then isostatic cool pressing forming of green body is carried out, forming pressure 140MPa ~ 200Mpa, 10 ~ 15 minutes dwell times;
(4), by step (3) gained formed material sinter, sintering schedule is for be warming up to 1700 DEG C ~ 1800 DEG C with stove, and be incubated 3 ~ 4 hours, stove is cold, final obtained yttria-stabilized zirconia crucible.
Described two Zirconium acetate agglutinate agent can produce chemical reaction with the oxidation zircon sand of stabilized with yttrium oxide under high temperature sintering condition, thus improve crucible purity and thermodynamic stability, and this is the feature not available for other binding agent.
In step (2), its grain size proportion of oxidation zircon sand of nodularization granulation gained stabilized with yttrium oxide is preferably weight ratio 1 ~ 2mm:0.5mm ~ 1mm: be less than 0.5mm=40 ~ 50:10 ~ 15:25 ~ 30.
Advantage of the present invention is:
1. the present invention adopts the zirconium white crucible of stabilized with yttrium oxide to have good thermodynamic stability, greatly reduce the reaction in metal liquid fusion process and between crucible, and the oxide inclusions content effectively reduced in alloy liquid, improves alloy purity and performance.
2. the present invention's positive pressure smelting 4J36 alloy under an inert atmosphere, effectively inhibits the volatilization of alloy liquid and splashes.
3. process for vacuum induction smelting of the present invention, equipment cost is low, and technique is simple, easy to operate, greatly reduces alloy manufacturing cost.
Embodiment
Embodiment of the present invention raw materials composition is in table 1:
Table 1 material composition
Yttria-stabilized zirconia crucible preparation process:
(1), get 320 order yttrium oxide powder and 320 order zirconia powders are raw material, the ratio being 8% yttrium oxide powder and 92% zirconia powder according to mass percent carries out mixing rear ball milling;
(2), high-temperature electric arc melting method is adopted to carry out high temperature sintering, sintering temperature 1800 DEG C, resulting materials carries out nodularization granulation, the oxidation zircon sand of obtained stabilized with yttrium oxide after screening, and wherein grain size proportion is weight ratio 1 ~ 2mm:0.5mm ~ 1mm: be less than 0.5mm=5:1.5:3;
(3), in the oxidation zircon sand of stabilized with yttrium oxide, the CaO particle that granularity is 1 ~ 3mm is added, two acetic acid zirconiums are added again after both mixing, wherein the weight percent of each composition is: the oxidation zircon sand of 93% stabilized with yttrium oxide, 5%CaO particle, 2% 2 acetic acid zirconium;
Isostatic cool pressing forming of green body, forming pressure 140MPa, 10 minutes dwell times;
(4), by step (3) gained formed material sinter, sintering schedule is for be warming up to 1750 DEG C with stove, and be incubated 4 hours, stove is cold, final obtained yttria-stabilized zirconia crucible, purity >=99.8%.
Embodiment 1
With the zirconium white crucible of thermodynamically stable stabilized with yttrium oxide, induction melting 4J36 low expansion alloy under malleation argon gas atmosphere, detailed process is:
1) alloy raw material: be electrolytic nickel 35% by mass percentage, electrolytic manganese 0.2%, alloy raw material got by pure iron 64.8%;
2) shove charge: the zirconium white crucible of stabilized with yttrium oxide put into by electrolytic nickel and pure iron, alloy secondary charging bucket put into by electrolytic manganese, adds after metallization in crucible is clear;
3) malleation is applied: first vacuumized by body of heater, when the low vacuum in stove is in 3Pa, applying argon gas in stove, plus-pressure is to 1000Pa;
4) alloy melting: power transmission, fusing pure iron and electrolytic nickel, in melting process, add electrolytic manganese in the zirconium white crucible of stabilized with yttrium oxide;
5) cast of alloy: all changed by described alloy raw material clearly, adjustment teeming temperature to 1500 DEG C, cast alloy liquid, obtain 4J36 alloy-steel casting, its foreign matter content is in table 2.
Embodiment 2
With the zirconium white crucible of thermodynamically stable stabilized with yttrium oxide, induction melting 4J36 low expansion alloy under malleation argon gas atmosphere, detailed process is:
1) alloy raw material: be electrolytic nickel 37% by mass percentage, electrolytic manganese 0.6%, alloy raw material got by pure iron 62.4%;
2) shove charge: the zirconium white crucible of stabilized with yttrium oxide put into by electrolytic nickel and pure iron, alloy secondary charging bucket put into by electrolytic manganese, adds after metallization in crucible is clear;
3) malleation is applied: first vacuumized by body of heater, when the low vacuum in stove is in 3Pa, applying argon gas in stove, plus-pressure is to 1500Pa;
4) alloy melting: power transmission, fusing pure iron and electrolytic nickel, in melting process, add electrolytic manganese in the zirconium white crucible of stabilized with yttrium oxide;
5) cast of alloy: all changed by described alloy raw material clearly, adjustment teeming temperature to 1560 DEG C, cast alloy liquid, obtain 4J36 alloy-steel casting, its foreign matter content is in table 2.
Embodiment 3
With the zirconium white crucible of thermodynamically stable stabilized with yttrium oxide, induction melting 4J36 low expansion alloy under malleation argon gas atmosphere, detailed process is:
1) alloy raw material: be electrolytic nickel 36.5% by mass percentage, electrolytic manganese 0.4%, alloy raw material got by pure iron 63.1%;
2) shove charge: the zirconium white crucible of stabilized with yttrium oxide put into by electrolytic nickel and pure iron, alloy secondary charging bucket put into by electrolytic manganese, adds after metallization in crucible is clear;
3) malleation is applied: first vacuumized by body of heater, when the low vacuum in stove is in 3Pa, applying argon gas in stove, plus-pressure is to 1200Pa;
4) alloy melting: power transmission, fusing pure iron and electrolytic nickel, in melting process, add electrolytic manganese in the zirconium white crucible of stabilized with yttrium oxide;
5) cast of alloy: all changed by described alloy raw material clearly, adjustment teeming temperature to 1530 DEG C, cast alloy liquid, obtain 4J36 alloy-steel casting, its foreign matter content is in table 2.
Comparative example 1
The crucible corundum ceramic crucible of melting, purity >=99.8%, induction melting 4J36 low expansion alloy under malleation argon gas atmosphere, detailed process is:
1) alloy raw material: get pure iron, electrolytic nickel, electrolytic manganese by the massfraction of 4J36 alloy requirement; Mass percent is electrolytic nickel 36.5%, electrolytic manganese 0.4%, pure iron 63.1%;
2) shove charge: corundum ceramic crucible put into by electrolytic nickel and pure iron, alloy secondary charging bucket put into by electrolytic manganese, adds after metallization in crucible is clear;
3) malleation is applied: first vacuumized by body of heater, when the low vacuum in stove is in 3Pa, applying argon gas in stove, plus-pressure is to 1200Pa;
4) alloy melting: power transmission, fusing pure iron and electrolytic nickel, in melting process, add manganese metal in corundum ceramic crucible;
5) cast of alloy: all changed by described alloy raw material clearly, adjustment teeming temperature to 1530 DEG C, cast alloy liquid, obtain 4J36 alloy-steel casting, its foreign matter content is in table 2.
Comparative example 2
Be to adopt different crucible for smelting 4J36 alloy from the difference of embodiment 1: adopt silicon sol as binding agent, raw material for crucible proportioning is weight percentage: 2% silicon sol, 93% yttria-stabilized zirconia sand, 5%CaO particle, adopt this crucible 4J36 alloy, obviously increased by the visible melting gained alloy impurity content of table 2.
Comparative example 3
Be to adopt different crucible for smelting 4J36 alloy from the difference of embodiment 1: this raw material for crucible proportioning is weight percentage: the oxidation zircon sand of 92% stabilized with yttrium oxide, 5%CaO particle, 3% 2 acetic acid zirconium, the crucible for smelting gained 4J36 alloy impurity content prepared as seen by table 2 obviously increases.
Table 2 4J36 alloy-steel casting foreign matter content (weight percent)
|
C |
Si |
P |
S |
Embodiment 1 |
0.01 |
0.01 |
0.004 |
0.004 |
Embodiment 2 |
0.01 |
0.013 |
0.003 |
0.003 |
Embodiment 3 |
0.012 |
0.012 |
0.003 |
0.004 |
Comparative example 1 |
0.03 |
0.20 |
0.01 |
0.01 |
Comparative example 2 |
0.01 |
0.35 |
0.004 |
0.004 |
Comparative example 3 |
0.04 |
0.01 |
0.004 |
0.004 |
Above-described embodiment, only for technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to spirit of the present invention change or modify, and all should be encompassed within protection scope of the present invention.